홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Water → 4'-Nitro-2-hydroxyacetophenone O-methyloxime

HRID 977068
노트
인쇄 미리보기

반응식

HRID 977068 반응식
Cl.[CH3:2][O:3][NH2:4].[N+:5]([C:8]1[CH:13]=[CH:12][C:11]([C:14](=O)[CH2:15][O:16][Si](C(C)(C)C)(C)C)=[CH:10][CH:9]=1)([O-:7])=[O:6].O1CCOCC1.O>CO>[CH3:2][O:3][N:4]=[C:14]([C:11]1[CH:10]=[CH:9][C:8]([N+:5]([O-:7])=[O:6])=[CH:13][CH:12]=1)[CH2:15][OH:16]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 312751,4-DioxaneHCID 521874O-Methylhydroxylamine hydrochlorideHCID 199641862-(Tert-butyldimethylsilyloxy)-1-(4-nitrophenyl)ethanone

생성물 1

HCID 542695314'-Nitro-2-hydroxyacetophenone O-methyloxime수율 67.3%

시약·촉매·용매 1

HCID 887
Methanol
용매

반응 조건

온도
80 °C

실험 절차

69 mg of O-methylhydroxylamine hydrochloride were added to a solution of 0.12 g (0.41 mmol) of 4'-nitro-2-t-butyldimethylsilyloxyacetophenone (obtained above) in a mixture of methanol (1.2 ml), 1,4-dioxane (2.0 ml) and water (2.0 ml). The resulting mixture was stirred for 1.5 hours at 80° C., then poured into water and extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The residue was purified by silica gel column chromatography, eluted with a stepwise gradient of ethyl acetate (10-40%) in hexane, to give 58 mg (67% yield) of the title compound.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with a saturated aqueous solution of sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe residue was purified by silica gel column chromatography
  5. washeluted with a stepwise gradient of ethyl acetate (10-40%) in hexane

출처 및 근거

ORD 기록
ord-fe6957ee84a24596bcaa962508debe81
출처 데이터셋
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05614470

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트